112results about "Ether preparation by compound dehydration" patented technology

The invention belongs to the technical field of organic synthesis, and relates to a preparation method of bis (trimethylolpropane), which comprises the following steps: preparing 2, 2-bis (hydroxymethyl) butyraldehyde from trimethylolpropane under the action of an oxidant; then, trimethylolpropane and 2, 2-bis (hydroxymethyl) butyraldehyde are subjected to reductive etherification under the action of a reductive etherifying agent and a catalyst, and the target product bis (trihydroxymethyl) propane is obtained. The preparation method of bis (trihydroxymethyl) propane has the advantages of few reaction steps and mild conditions, can improve the reaction yield, and is beneficial to the realization of industrial application.

A method for producing a (poly)alkylene glycol monoalkyl ether includes reacting an olefin and a (poly)alkylene glycol in a reactor in a presence of a catalyst. The method also includes recovering at least a portion of raw materials used for the production to use the recovered raw materials again as a raw material, where at least one of the recovered raw materials contains an olefin. A mass of a branched olefin relative to a mass sum of the branched olefin and a linear olefin contained in the recovered raw materials is controlled not to exceed 20 mass %.

The invention relates to a dapagliflozin impurity and a preparation method thereof, 5-bromo-2-chlorobenzoic acid (IV) is used as a raw material, (5-bromo-2-chlorphenyl) (4-ethyoxyl phenyl) ketone (III) is prepared through chlorination and Friedel-Crafts acylation, (5-bromo-2-chlorphenyl) (4-ethyoxyl phenyl) methanol (II) is obtained through reduction, and the benzhydryl ether impurity (I) is obtained through condensation under the catalysis of iodine. The preparation method has the advantages of simple operation, low cost, easily available raw materials and good product purity.

In order to overcome the problems of high recovery price, high energy consumption and low utilization rate of the existing kettle residue for the production of ethylene glycol by ethylene carbonate alcoholysis method, the application provides a kettle residue recovery method and device for the production of ethylene glycol by ethylene carbonate alcoholysis method, and the application provides a kettle residue recovery method for the production of ethylene glycol by ethylene carbonate, which comprises the following steps: under the conditions of temperature 150-250 DEG C and pressure 0.6-2 MPa, the ethylene glycol in the kettle residue produced by the preparation of ethylene glycol by ethylene carbonate alcoholysis method is converted into diethylene glycol under the catalysis of alkali metal salt catalyst, and after the reaction is completed, the kettle residue is a mixture of ethylene glycol, diethylene glycol, triethylene glycol and salt, the mixture is purified, and ethylene glycol and diethylene glycol are recovered; the economic benefit is improved, the rectification separation operation is simplified, the equipment investment and the overall energy consumption are reduced, and the utilization rate of ethylene glycol kettle residue is improved.

The device comprises an ethylene glycol storage tank (1), a nitrogen storage tank (2), a mixed gas storage tank (3), a high-pressure plunger pump (4), a preheater (7), a mass flow meter (8), a fixed bed reactor (9), a condenser (10), a phase splitter (11), a liquid collection tank (12), a gas chromatograph (14), a back pressure valve (16), a liquid chromatograph (17) and a plurality of valves. The ethylene glycol storage tank (1) is sequentially connected with the high-pressure plunger pump (4), the preheater (7), the fixed bed reactor (9), the condenser (10) and the phase splitter (11); and the nitrogen storage tank (2) is sequentially connected with a valve (5), the mass flow meter (8) and the preheater (7). By regulating and controlling the acidity and pore channel structure of the molecular sieve, efficient synthesis of the low polyethylene glycol is realized, and the problem of low product selectivity in similar catalysts is solved.

The invention relates to a catalyst for preparing anisole through phenol methanol etherification as well as a preparation method and application of the catalyst. The catalyst takes aluminum phosphate as a carrier and is doped with zirconium oxide; on the basis of the mole number of Al, the mole ratio of P to Al is (0.05-2): 1, and the mole ratio of Zr to Al is (0.08-0.20): 1. Dropwise adding the aluminum-zirconium mixed aqueous solution into the phosphorus source aqueous solution, stirring, standing and washing to obtain a solid sample; and drying and roasting the solid sample to obtain the aluminum phosphate catalyst. Under the action of the catalyst, phenol and methanol are catalyzed to generate anisole. Compared with the prior art, the phenol conversion rate is greater than or equal to 50%, the anisole selectivity is greater than or equal to 85%, highly toxic dimethyl sulfate and a large amount of alkali are not needed, the process is green, the cost is low, separation is simple, and the method is suitable for large-scale industrial production of anisole.

The invention discloses a preparation method of Linzagolix, which comprises the following steps: taking 2, 3-difluoro-6-methoxybenzyl alcohol as a raw material, under the action of alkali and phosphine ligand, carrying out Mitsunobu reaction on 2, 3-difluoro-6-methoxybenzyl alcohol and 2-methoxy-4-fluorophenol to obtain a compound A, sequentially carrying out nitration reaction and reduction reaction on the compound A to obtain a compound C, and carrying out recrystallization on the compound C to obtain the Linzagolix. Under the alkaline condition and the action of triphosgene, the compound C and 4-aminothiophene-2, 3-dimethyl dicarboxylate hydrochloride are subjected to a one-pot condensation reaction to obtain a compound D, and the compound D reacts under the alkaline condition to generate Linzaolix. According to the invention, the synthesis process of Linazagolix is shortened to five steps, the reaction condition is mild, the operation is simpler and more convenient, and the method is suitable for industrial production.

The invention discloses preparation and application of a diethylene glycol etherification catalyst, and belongs to the technical field of organic synthesis. The catalyst disclosed by the invention is prepared by loading metal M into pores of an acidic molecular sieve and then roasting, the metal M is one or more than two of Fe, Co, Ni, Cu, Zn, Nb, Ag, Sn, W, Ga, Pd, Re, Y, La, Ce, Nd, In, Zr, Sm and Er, and the content of the metal M in the catalyst is 0.1-50 wt%; the catalyst is used in a reaction for catalyzing diethylene glycol and low-carbon alcohol to prepare diethylene glycol ether, the selectivity of the diethylene glycol ether is remarkably improved, and the catalyst is low in raw material cost, simple in preparation method, easy to industrially amplify and very good in application prospect.

To improve the recovery rate of alcohol, which is a constituent monomer of polyester resin, in a method for decomposing polyester resin using high-temperature water. [Solution] A method for decomposing polyester resin, comprising step (i) of hydrothermally treating polyester resin in the presence of polyamide resin, wherein step (i) includes proceeding with hydrolysis of the polyester resin at a temperature of 150°C or higher.

The invention relates to the technical field of coal chemical industry and discloses a reaction device and method for dimethyl ether carbonylation and ethylene glycol catalytic conversion, and the reaction device comprises a reactor, a first buffer tank, a dimethyl ether pipeline, a liquid storage tank and a nitrogen pipeline, a mixed gas formed by carbon monoxide and hydrogen is contained in the first buffer tank, the dimethyl ether pipeline is used for supplying a dimethyl ether raw material to the reactor, the dimethyl ether raw material, the mixed gas and a first catalyst can perform dimethyl ether carbonylation reaction, mixed alcohol formed by ethylene glycol and methanol is contained in the liquid storage tank, and the liquid storage tank is used for supplying the mixed alcohol to the reactor. And the nitrogen pipeline is communicated with the reactor so as to purge the reacted reactor and supply nitrogen required by the ethylene glycol catalytic conversion reaction. According to the reaction device for carbonylation of dimethyl ether and catalytic conversion of ethylene glycol in the embodiment of the invention, two reactions are carried out through the same reactor, and two sets of complete reaction devices do not need to be additionally built.

The invention belongs to the technical field of catalytic reaction and separation and purification, and particularly relates to a preparation method of isotope dimethyl ether. The method comprises the following steps: by taking a mixture of a metal oxide nanosheet and a nanosheet-shaped ZSM-5 molecular sieve as a catalyst, carrying out dehydration reaction on isotope methanol under the action of the catalyst; after the reaction is finished, a reaction product enters a U-shaped pipe filled with a water absorption drying agent, is subjected to first-stage separation and purification in an ice salt bath environment, then enters an adsorption bottle I, is subjected to second-stage separation and purification in a liquid nitrogen and ethanol mixed bath environment, and then enters an adsorption bottle II; third-stage separation and purification are carried out in a liquid nitrogen and isopropanol mixed bath environment, finally, reaction products enter an absorption bottle III, and fourth-stage separation and purification are carried out in the liquid nitrogen and isopropanol mixed bath environment. The method provided by the invention can realize high-conversion-rate and high-selectivity generation of dimethyl ether from methanol, and realizes 100% isotope methanol recovery efficiency and 100% separation and collection of isotope dimethyl ether.

The present invention relates to a process for the preparation of (4Z)-11,11-dialkoxy-4-undecenyl triaryl phosphonium halides of general formula (3-Z), wherein Y represents a halogen atom, Ar represents independently of each other an aryl group, R 1 and R 2 represent independently of each other a monovalent hydrocarbon group having 1 to 15 carbon atoms, or R 1 and R 2 may together form a divalent hydrocarbon group R 1 -R 2 having 2 to 10 carbon atoms, which process comprises: subjecting a (7Z)-11-halo-1,1-dialkoxy-7-undecene compound of general formula (1-Z), wherein X 1 represents a halogen atom, R 1 and R 2 are as defined above, to a phosphonium salt forming reaction with a phosphine compound of general formula (2), wherein Ar is as defined above, to form said compound (3-Z); and also relates to a compound of general formula (A) L(CH2)3CH=CH(CH2)5CH(OR 1 )(OR 2 )(A), wherein R 1 and R 2 are as defined above.

The present disclosure provides a method of preparing olefins from methanol, in which methanol and phenol-like molecules are used as raw material, which is gasified and then passed into a two-stage fixed-bed catalytic reactor. The raw material reacts with a catalyst A (silica-aluminum molecular sieve) and a catalyst B (silica-aluminum or phosphorus-aluminum molecular sieve) in sequence to produce ethylene. The method of the present disclosure has a high selectivity, which using phenol-like molecules as a molecular catalyst, and a catalytic reaction by co-feeding methanol and the phenol-like molecules. After gasification of the raw material, the raw material is brought into the reactor by an inert gas, and after a two-stage catalyst system, the selectivity of ethylene reaches more than 90%, which solves the problem of the products separation in the current process. In addition, the process described in the present disclosure has a good stability. A little coke is formed in catalyst during the reaction, which solves the problem that the catalyst is required to be regenerated repeatedly.

The invention discloses a catalyst for preparing 1-octene or octyl ether through dehydration of 1-octanol, the catalyst is a gradient acid site catalyst, and the total proportion of weak acid sites and medium-strong acid sites of the catalyst is greater than or equal to 70%; the catalyst is composed of a carrier, P2O5 and ZnO, wherein the P2O5 and the ZnO are loaded on the carrier, and the carrier is gamma-Al2O3; according to the mass of the gamma-Al2O3, the loading capacity of the ZnO is 2-5%, and the loading capacity of the P is 0.5-1.0%. Meanwhile, the invention discloses a preparation method and application of the catalyst. The total proportion of the catalyst, the weak acid site and the medium-strong acid site is greater than or equal to 70%, the catalyst is a gradient acid site catalyst, the weak acid site can promote intermolecular dehydration to generate octyl ether, and the medium-strong acid site can promote intramolecular dehydration to generate 1-octene, so that the catalyst realizes dual purposes.

The invention discloses vanillyl butyl ether and a synthesis method thereof, and relates to the technical field of synthesis of vanillyl butyl ether.The synthesis method of vanillyl butyl ether comprises the following steps that S1, vanillyl alcohol is prepared; s2, adding vanillyl alcohol prepared in the step S1, n-butyl alcohol and a catalyst into a reaction kettle, and uniformly stirring to react, so as to obtain a mixed solution after the reaction is completed; s3, filtering the mixed solution prepared in S2, pretreating filtrate, and extracting an organic phase in the filtrate; s4, carrying out primary reduced pressure distillation on the organic phase extracted in S3 to obtain a vanillyl butyl ether crude product and n-butyl alcohol, then recovering n-butyl alcohol, and carrying out secondary reduced pressure distillation on the vanillyl butyl ether crude product to obtain vanillyl butyl ether; the whole synthesis method is low in raw material cost, mild in reaction condition, simple in process and small in wastewater generation amount, recycling of the catalyst and the solvent is achieved, the prepared vanillyl butyl ether is large in yield and high in purity, a brand new solution is provided for efficient and green production of the vanillyl butyl ether, and industrial popularization is facilitated.

Methods and systems or devices for synthesis of valuable chemicals from carbon dioxide and hydrogen are provided. A high surface area hollow fiber catalytic membrane reactor such as with hollow fibers coated with a water permeable membrane material is used. The reactor also contains methanol synthesis component, and as needed, a dehydration catalyst component such that the two-step reaction takes place on the catalyst surface. Produced water permeates through the membrane, exiting the reactor immediately after it is formed. Unreacted reactants and products flow to the reactor exit. The valuable chemicals can be liquefied petroleum gas (LPG), dimethyl either (DME), methanol, ethanol, olefin, jet fuel or a combination thereof.

This invention relates to the fields of materials science and chemistry, and discloses a method for preparing a metal ion-doped defective FER molecular sieve. The method includes a molecular sieve using Cu and Co as doping ions, with a basic framework of a defective FER molecular sieve having a silicon-to-aluminum ratio of 30-40. The molecular sieve is based on the mass of the defective FER molecular sieve, and the mass percentage of the doping ions is 3-5%. This invention employs a two-step synthesis method. The first step involves hydrothermal crystallization to synthesize a pre-crystallized FER molecular sieve. The second step increases the hydrothermal crystallization temperature, causing the unstable molecular sieve structure to transform into a high silicon-to-aluminum ratio defective crystal form under high temperature and pressure, while simultaneously introducing heteroions into the molecular sieve framework. Compared to traditional techniques, this method can achieve a larger doping amount and is simpler with readily available raw materials. Its application in the catalytic synthesis of ethylene glycol dimethyl ether from ethylene glycol and methanol can achieve high conversion rates and high selectivity, demonstrating significant economic value and market potential.

The present invention relates to a method for the preparation of bisphenol-A for the synthesis of polycarbonate according to claim 1, and to a method for the preparation of polycarbonate from the bisphenol-A obtained according to the above-mentioned preparation method according to claim 14, and to a multi-component system for the preparation of bisphenol-A according to the above-mentioned preparation method. In this method, the bisphenol-A is prepared from provided acetone and provided phenol, wherein these raw materials have to be method products of a specific preparation method which are based on CO2, methane from a biological source, carbohydrates and / or organic, solid compounds as starting materials.

The invention discloses vanillin alcohol ether and a preparation method thereof, and the preparation method comprises the following steps: (1) by taking vanillin or ethyl vanillin and hydrogen as reactants and alcohol or ethyl acetate (EA) as a solvent, preparing a reactant solution, adding a Raney nickel catalyst as a catalyst, and reacting at the temperature of 40-70 DEG C under the reaction hydrogen pressure of 2-3 MPa for 8-10 hours; and (2) by taking vanillin alcohol or ethyl vanillin alcohol and second alcohol as reactants and lewis acid (such as magnesium chloride, aluminum chloride, calcium chloride, ferric chloride, copper sulfate and other lewis acids) as a catalyst, reacting at 80-100 DEG C to obtain vanillin alcohol ethers, the preparation method disclosed by the invention is mild in reaction condition, few in by-products, green and environment-friendly, high in product yield and suitable for industrial production.

A method for producing alkyl ethers, the method comprising: feeding a hydrocarbon feedstock and a first alcohol feedstock to a fixed bed reactor containing an etherification catalyst. The hydrocarbon feedstock and the first alcohol feedstock are contained in the first fixed bed reactor, and react an isoolefin with an alcohol in the presence of an etherification catalyst to produce a first product stream. The first product stream is fed together with a hydrogen feedstock and a second alcohol feedstock to a catalytic distillation reaction system, the catalytic distillation reaction system containing a trifunction catalyst, thereby simultaneously isomerizing at least a portion of the α-olefins, hydrogenating at least a portion of the diolefins, and etherifying at least a portion of the isoolefins and the alcohol to produce a bottoms product and an overhead product. The bottoms product comprises one or more ethers. The overhead product comprises n-alkanes, isoalkanes, unreacted α-olefins, unreacted internal olefins, unreacted isoolefins, and unreacted alcohol.

The invention provides a method for preparing vinyl ether by cracking ethylene glycol monoether or / and diether, which comprises the following steps of: loading ethylene glycol monoether, diether or mixed ether with a structural formula of HOCH2CH2OR or / and ROCH2CH2OR (R is alkyl or substituted alkyl) into a fixed bed reactor bed layer of a supported Cs-series and Ca-Mg-series solid base catalyst through mixing, layering or bed separation; reacting to generate a vinyl ether gas-phase mixture with a structural formula of CH2 = CHOR, and then treating a cracking reaction product through a gas-liquid separation process and a separation refining process to obtain the high-purity vinyl ether. The method provided by the invention adopts a continuous reaction process, the device can be large-scale, the operation is simple and convenient, and the process is safe and environment-friendly; the ethylene glycol mono / di-mixed ether crude raw material without separation can be used, the cracking reaction activity of ethylene glycol ether and the selectivity of vinyl ether are high, the performance of the catalyst is stable, and the production cost is low.

The present disclosure generally relates to the synthesis of an alkoxylated cannabinoid using a double metal cyanide (DMC) catalyst. This procedure affords a novel process for preparing water-dispersible and water-soluble versions of cannabidiol (CBD) and other cannabinoids in high yields through mild reaction conditions.

Provided are a polyhydroxy aromatic intermediate, preparation thereof and use thereof in a polycondensate water-reducer with branched side chains. The polycondensate water-reducer with branched side chains has a branched side chain structure which provides a stronger steric hindrance. The synergistic effect of the branched side chains and the rigid skeleton of the aromatic ring greatly improves the water-reducing ability. Especially under a condition of low water / cement ratio, the improvement in water-reducing ability is more obvious. The branched polyether side chain is more conducive to the formation of a thicker water film layer, which has an obvious viscosity reduction effect. The conformation of the branched polyether side chain is less affected by different ionic environments in the pore solution in cement, and thus has a stronger adaptability to various raw materials. The water-reducer is suitable for the preparation of high-strength concrete, self-compacting concrete and concrete with low water-to-binder ratio and high volume of mineral admixtures, especially for the preparation of concrete containing machine-made sand.

The invention belongs to the technical field of high-value utilization of organic wastes, and particularly relates to a method for high-value utilization of phenolic tar. According to the method, the phenol tar is subjected to alcoholysis, alkylation, steam stripping, rectification, melt crystallization purification and other procedures to obtain high-added-value fine chemical products such as p-xylylene ether and anisole, and the residual tar after steam stripping can be continuously used as fuel to be incinerated to produce steam. According to the method disclosed by the invention, the hydroquinone in the phenol tar can be reacted and converted, the phenol tar with low polymerization degree can be alcoholyzed into phenol, hydroquinone and a small amount of catechol, part of phenolic compounds can be etherified with methanol and then converted into p-xylylene ether and anisole through alkylation, and according to measurement and calculation, the content of the p-xylylene ether in the phenol tar can be measured and calculated, and the content of the p-xylylene ether in the phenol tar can be measured and calculated. According to hydroquinone corresponding to the generated p-xylylene ether, the phenol tar can be converted into hydroquinone with the weight being 10% or above of the weight of tar through alcoholysis by deducting the original hydroquinone amount in the phenol tar, and therefore high-value utilization of the phenol tar is achieved.

The invention relates to the technical field of fine chemical engineering, and provides a method for synthesizing dipentaerythritol and a composite material thereof. The amino-rich mesoporous molecular sieve and alkaline oxide are mixed in proportion to adsorb formaldehyde, and the reversible formaldehyde-loaded composite material is obtained. In the reaction process, acetaldehyde or acetaldehyde-formaldehyde mixed liquid is put into a reactor at a time, the composite material is added, then alkali liquor is added into a system continuously or in batches at a controlled rate, formaldehyde is slowly released from the composite material and enters the reaction system, condensation reaction is conducted on the formaldehyde and acetaldehyde under the low-temperature condition, and dipentaerythritol is directionally generated. After the reaction is finished, the composite material is filtered and recycled, and can be recycled after being roasted.

The application belongs to the technical field of MTBE synthesis catalysts, and particularly relates to an MTBE synthesis catalyst, a preparation method and application thereof. The preparation method of the MTBE synthesis catalyst comprises the following steps: an oil phase composed of styrene, methyl methacrylate, divinylbenzene, a pore former and an initiator, and an aqueous phase composed of water, a dispersing agent and a co-dispersing agent are subjected to suspension copolymerization, and then the MTBE synthesis catalyst is prepared through solidification, pore former removal, drying and screening of a sulfonated matrix prepared through the above steps, and then through sulfonation, acid washing and water washing. The MTBE synthesis catalyst has suitable particle size, suitable pore structure and high exchange equivalent, and the hydrophobic groups on the white balls can timely remove the generated water from the reaction system, so that the MTBE synthesis catalyst has a good application prospect in the application field of synthesizing methyl tert-butyl ether from tert-butyl alcohol and methanol.

The application discloses a preparation method of polyglycerol and belongs to the technical field of fine chemical synthesis; in the preparation method of polyglycerol, polystyrene microspheres loaded with phosphomolybdic acid and gallium oxide are introduced as a solid acid catalyst, the phosphomolybdic acid, the gallium oxide and the polystyrene microspheres can interact with each other, so that the reaction efficiency of glycerol polymerization is remarkably improved, and further by controlling the reaction temperature and the reaction time, the polyglycerol with high purity and high yield can be synthesized; and the polyglycerol obtained has light color and high quality. Meanwhile, in the preparation method, the reaction temperature is relatively low, the energy consumption is small, the solid acid catalyst used can be separated by filtration and recycled, the green and environmental protection effect is achieved, and in addition, in the preparation method, no toxic, harmful or highly corrosive substances are used, so that the safety in the preparation process can be effectively ensured.

The present invention discloses SCM-38 molecular sieve, its preparation method and its use. SCM-38 molecular sieve is phosphorus-aluminum or silicon-phosphorus-aluminum molecular sieve. XRD spectrum of SCM-38 molecular sieve shows X-ray diffraction peaks at 2θ of 7.20±0.1, 10.81±0.1, 11.60±0.1, 14.32±0.1, 21.39±0.1, 21.83±0.1, 27.31±0.1 and 28.72±0.1, and has the most intense peak at 2θ of 7.20±0.1. SCM-38 molecular sieve of the present invention can be used in catalyst.

To provide a solid-supported ruthenium complex useful as a catalyst for producing allyl compounds, a method for producing the same, and a method for producing an allyl compound using the same.SOLUTION: The solid-supported ruthenium complex is represented by General Formula (1), and an allyl compound is produced using the solid-supported ruthenium complex as a catalyst.SELECTED DRAWING: None

This invention provides a method for synthesizing ethyl vanillin, belonging to the field of efficient chemical synthesis technology. The method includes the following steps: (1) under a protective atmosphere, catechol, ethanol, and Nb₂O₅ are mixed and subjected to an etherification reaction to obtain o-ethoxyphenol; (2) under a protective atmosphere, o-ethoxyphenol, formaldehyde solution, and Mo₂C are mixed and subjected to an addition reaction to obtain 3-ethoxy-4-hydroxybenzyl alcohol; (3) 3-ethoxy-4-hydroxybenzyl alcohol, water, and MnO₂ are mixed and subjected to an oxidation reaction to obtain the ethyl vanillin. This invention employs a heterogeneous catalytic reaction process, using Nb₂O₅, Mo₂C, and MnO₂ as solid catalysts. The catalysts are easily separated and recovered from the reaction system. Furthermore, the entire process does not use highly corrosive substances such as hydrochloric acid and sodium hydroxide, nor homogeneous catalysts such as phase transfer catalysts. Compared to traditional homogeneous reaction synthesis techniques, the process is green and environmentally friendly, with excellent yield and conversion rates.